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Li+- and Eu3+-Doped Poly(ε-caprolactone)/Siloxane Biohybrid Electrolytes for Electrochromic Devices

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† Department of Chemistry and CQ-VR, University of Trás-os-Montes e Alto Douro, 5001-801 Vila Real, Portugal
‡ Department of Physics and CICECO, University of Aveiro, 3810-193 Aveiro, Portugal
⊥ Department of Chemistry, University of Minho, Gualtar, 4710-057 Braga, Portugal
# CENIMAT/I3N, Departamento de Ciência dos Materiais, Faculdade de Ciências e Tecnologia, FCT, Universidade Nova de Lisboa and CEMOP-UNINOVA, 2829-516 Caparica, Portugal
Phone: 00-351-259350253. Fax: 00-351-259350480. E-mail: [email protected]
Cite this: ACS Appl. Mater. Interfaces 2011, 3, 8, 2953–2965
Publication Date (Web):July 20, 2011
https://doi.org/10.1021/am200391b
Copyright © 2011 American Chemical Society
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    Abstract

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    The sol–gel process has been successfully combined with the “mixed cation” effect to produce novel luminescent and ion conducting biohybrids composed of a diurethane cross-linked poly(ε-caprolactone) (PCL530)/siloxane hybrid network (PCL stands for the poly(ε-caprolactone) biopolymer and 530 is the average molecular weight in gmol–1) doped with a wide range of concentrations of lithium and europium triflates (LiCF3SO3 and Eu(CF3SO3)3, respectively) (molar ratio of ca. 50:50). The hybrid samples are all semicrystalline: whereas at n = 52.6 and 27.0 (n, composition, corresponds to the number of (C(═O)(CH2)5O) repeat units of PCL(530) per mixture of Li+ and Eu3+ ions) a minor proportion of crystalline PCL(530) chains is present, at n = 6.1, a new crystalline phase emerges. The latter electrolyte is thermally stable up to 220 °C and exhibits the highest conductivity over the entire range of temperatures studied (3.7 × 10–7 and 1.71 × 10–4 S cm–1 at 20 and 102 °C, respectively). According to infrared spectroscopic data, major modifications occur in terms of hydrogen bonding interactions at this composition. The electrochemical stability domain of the biohybrid sample with n = 27 spans more than 7 V versus Li/Li+. This sample is a room temperature white light emitter. Its emission color can be easily tuned across the Commission Internationale d’Éclairage (CIE) chromaticity diagram upon simply changing the excitation wavelength. Preliminary tests performed with a prototype electrochromic device (ECD) comprising the sample with n = 6.1 as electrolyte and WO3 as cathodically coloring layer are extremely encouraging. The device exhibits switching time around 50 s, an optical density change of 0.15, good open circuit memory under atmospheric conditions (ca. 1 month) and high coloration efficiency (577 cm2 C–1 in the second cycle).

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